CN105788791B - Rare earth permanent magnet powder and preparation method thereof - Google Patents
Rare earth permanent magnet powder and preparation method thereof Download PDFInfo
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- CN105788791B CN105788791B CN201410835112.9A CN201410835112A CN105788791B CN 105788791 B CN105788791 B CN 105788791B CN 201410835112 A CN201410835112 A CN 201410835112A CN 105788791 B CN105788791 B CN 105788791B
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Abstract
The present invention provides a kind of rare earth permanent magnet powder and preparation method thereof, the key component of the rare earth permanent magnet powder is MMxFe1‑x‑yBy, wherein MM is norium, and x is 23~35wt%, and y is 0.95~1.05wt%；Rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, principal crystalline phase MM2Fe14B phases, and in richness MM phases La content of the content higher than La in principal crystalline phase, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.The norium has the rare earth elements such as Nd, Ce and the La directly isolated from primary mineral products, and has high magnetic property, to make the rare earth permanent magnet powder have high cost performance.
Description
Technical field
The present invention relates to permanent-magnet material technical fields, in particular to a kind of rare earth permanent magnet powder and preparation method thereof.
Background technology
Bonding rare earth permanent magnet material has been widely used for the various necks such as IT, automation, household electrical appliances by development for many years
Domain.The binding electromagnetic material being widely used at present is NdFeB materials, and preparation method mainly isolates rare earth from Rare Earth Mine
Metal obtains bonded permanent magnet powder after then carrying out mixed smelting, powder processed with Fe and B.
A large amount of uses of neodymium metal (Nd), keep the application of rare earth element extremely uneven in NdFeB materials.Currently, usually
The light rare earths such as La, Ce are added in NdFeB materials to improve its magnetic property and application characteristic, to generate different magnetic property gradients
Permanent-magnet material.For example, the Chinese patent of Publication No. CN100416719C discloses a kind of rare earth permanent-magnetic material, within this material
By adding rare earths and other magnesium-yttrium-transition metals such as La, Ce, Y, to reduce its magnetic property；But the element of this kind of method addition
It is numerous, while some nonmagnetic elements are artificially added in order to reach the ferritic purpose of replacement, to cause magnetism
The waste of energy.For another example the Chinese patent of Publication No. CN103714928A by the way that Ce is added in NdFeB, can prepare cerium
Iron-base permanent-magnet powder and the two kinds of magnetic powders of Re '-Fe-B for being free of Ce, however, to ensure that magnetic property also added heavy rare earth Dy, Tb etc.,
To cause economic waste, and the magnetic property of prepared magnetic powder is not also high.
However, after the light rare earths such as La, Ce are added in NdFeB materials, due to the intrinsic magnetic characteristic of light rare earth and neodymium metal
It differs greatly so that the magnetic property of magnetic powder is uneven and poor.Moreover, because existing rare earth permanent magnet powder is by from Rare Earth Mine
Light rare earth metal (Ce etc.) is isolated, is then added what the light rare earth metal isolated was formed in NdFeB again, therefore repeat numerous
The expensive rare earth metal of trivial processing step and addition can cause the waste of rare earth resources, and to various rare earths
The cost of preparation process can be also significantly increased in the separation of metal, and the cost performance so as to cause the rare earth permanent magnet powder of formation is very low.
Invention content
The main purpose of the present invention is to provide a kind of rare earth permanent magnet powders and preparation method thereof, in the prior art to solve
The low problem of the cost performance of rare earth permanent magnet powder.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of rare earth permanent magnet powder, the rare earth permanent magnet
The key component of powder is MMxFe1-x-yBy, wherein MM be norium, x be 23~35wt%, y be 0.95~
1.05wt%；Rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, principal crystalline phase MM2Fe14B phases, and
Content of the content of La higher than La in principal crystalline phase in rich MM phases, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Further, Ce contents are more than 48wt% in MM, and La contents are more than 15wt% in MM.
Further, T is contained in rare earth permanent magnet powder, wherein T is Co, Al, Zr and Si any one or more of, with rare earth
The gross mass of permanent magnetism powder key component calculates, and the percentage composition of T is 0.32~12.67wt%.
Further, the mass ratio of the T in rare earth permanent magnet powder and Fe is 0.5~10：100.
Further, the mass ratio of the T in rare earth permanent magnet powder and Fe is 0.5~5：100.
According to another aspect of the present invention, provide a kind of preparation method of rare earth permanent magnet powder, the preparation method include with
Lower step：Melting will be carried out to form key component as MMxFe1-x- with the mixed metal of MM, Fe and the B mixed in proportion
The master alloy of yBy, wherein MM are norium, and x is 23~35wt.%, and y is 0.95~1.05wt%；By master alloy into
Row fusing is to form molten alloy；Rotation is carried out to molten alloy and quenches processing to form alloy powder；And alloy powder is carried out
For rotation cooling treatment to form rare earth permanent magnet powder, rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase,
Principal crystalline phase is MM2Fe14B phases, and in richness MM phases La content of the content higher than La in principal crystalline phase, the content height of Pr in rich MM phases
In the content of principal crystalline phase Pr.
Further, molten alloy is sprayed onto on the roller of rotation and revolve processing of quenching, the linear velocity of roller is 20
~35m/s.
Further, the surface of roller is Mo layers or BeCu layers.
Further, in carrying out the step of rotation cooling treatment is to form rare earth permanent magnet powder to alloy powder, alloyed powder
The rotary speed at end is less than 5m/s.
Further, in the step of being melted master alloy, master alloy further includes T, and wherein T is Co, Al, Zr and Si
Any one or more of is calculated with the gross mass of rare earth permanent magnet powder key component, and the percentage composition of T is 0.32~
12.67wt%.
Further, the mass ratio of T and Fe is 0.5~10 in master alloy：100.
According to another aspect of the present invention, a kind of bonded permanent magnet is provided, which is above-mentioned rare earth permanent magnet powder
It is bonded with binder.
According to another aspect of the present invention, a kind of device is provided, which applies above-mentioned bonded permanent magnet.
It applies the technical scheme of the present invention, is MM the present invention provides a kind of key componentxFe1-x-yByRare earth permanent magnet
Powder, since the norium in the rare earth permanent magnet powder has Nd, Ce and La etc. for directly being isolated from primary mineral products
Rare earth element, therefore compared with the rare earth permanent magnet powder being made of the mixture of single rare earth metal and single rare earth metal, this
The rare earth permanent magnet powder that invention provides drastically reduces the waste of rare earth resources, and these rare earths member that norium has
The symbiotic characteristic of element makes it have apparent synergistic effect, so as to make rare earth permanent magnet powder show the permanent magnetism of single compound
Characteristic；Also, since the MM contents in the rare earth permanent magnet powder are 23%~35wt%, to make to form one in rare earth permanent magnet powder
Quantitative rich MM phase structures, richness MM phase structures can not only improve the coercivity of rare earth permanent magnet powder, and can become rare earth
Pinning sites of the permanent magnetism powder in reverse magnetization process to improve the magnetic property of the rare earth permanent magnet powder, and then make the rare earth forever
Magnetic powder has higher cost performance.
Specific implementation mode
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
MM provided by the present invention refers to norium known in those skilled in the art, by Rare Earth Mine
It extracts containing the yttrium and group of the lanthanides in the IIIth B races such as lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd) and a small amount of samarium (Sm), yttrium (Y)
The oxide or chloride of element mixing, and the norium is made through molten-salt electrolysis, and it is dilute in the norium
The total amount of earth metal is more than 98wt.%.
By background technology it is found that the cost performance of existing rare earth permanent magnet powder is very low.The present inventor is regarding to the issue above
It is studied, provides a kind of rare earth permanent magnet powder.The key component of the rare earth permanent magnet powder is MMxFe1-x-yBy, wherein MM is mixing
Rare earth metal, x are 23~35wt%, and y is 0.95~1.05wt%；Rare earth permanent magnet powder include principal crystalline phase and be distributed in principal crystalline phase week
The rich MM phases enclosed, principal crystalline phase MM2Fe14B phases, and in richness MM phases La content of the content higher than La in principal crystalline phase, in rich MM phases
The content of Pr is higher than the content of principal crystalline phase Pr.
Due to the norium in the rare earth permanent magnet powder have Nd, Ce for directly being isolated from primary mineral products and
The rare earth elements such as La, therefore the rare earth permanent magnet powder phase formed with the mixture by single rare earth metal and single rare earth metal
Drastically reduce the waste of rare earth resources than, rare earth permanent magnet powder provided by the invention, and norium have these
The symbiotic characteristic of rare earth element makes it have apparent synergistic effect, so as to make rare earth permanent magnet powder show single compound
Magnetic property；Also, since the MM contents in the rare earth permanent magnet powder are 23%~35wt%, to make shape in rare earth permanent magnet powder
At a certain amount of richness MM phase structures, richness MM phase structures can not only improve the coercivity of rare earth permanent magnet powder, and can be at
The pinning sites for being rare earth permanent magnet powder in reverse magnetization process, to improve the magnetic property of the rare earth permanent magnet powder, and then make this
Rare earth permanent magnet powder has higher cost performance.
The key component of rare earth permanent magnet powder provided by the invention is MMxFe1-x-yBy.Wherein, MM is norium, is led to
It crosses in Rare Earth Mine and extracts containing in the IIIth B races such as lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd) and a small amount of samarium (Sm), yttrium (Y)
Yttrium and lanthanide series mixing oxide or chloride, and made through molten-salt electrolysis, and the metal middle rare earth metal is total
Amount is more than 98wt.%.Since norium is to be separated from primary mineral products, and by single rare earth metal
And the rare earth permanent magnet powder of the mixture composition of single rare earth metal is compared, rare earth permanent magnet powder provided by the invention is greatly reduced
The wastes of rare earth resources.Also, due to norium directly from primary ore electrolytic separation and go out, mischmetal
The symbiotic characteristic of element is with apparent synergistic effect in metal, so as to make the rare earth permanent magnet powder of preparation show list
The magnetic property of one compound.
It is MM in key component provided by the inventionxFe1-x-yByRare earth permanent magnet powder in, x is 23~35wt%, and y is
0.95~1.05wt%.Since the MM contents in the rare earth permanent magnet powder are 23%~35wt%, so as to make rare earth permanent magnet powder
Middle to form a certain amount of richness MM phase structures, richness MM phase structures can not only improve the coercivity of rare earth permanent magnet powder, and can
As the pinning sites in rare earth permanent magnet powder reverse magnetization process, to improve the magnetic property of the rare earth permanent magnet powder；It is certain simultaneously
The B content of amount is to form MM2Fe14Element necessary to B principal crystalline phases.The B content energy of 0.95~1.05wt% in rare earth permanent magnet powder
Enrichments of the excessive B in rich MM phases is enough avoided, to be conducive to promote the whole magnetic property of rare earth permanent magnet powder.
It is further preferable that x is 25~32wt%.It, can when the content of MM in rare earth permanent magnet powder is 25%~32wt%
Coercitive decline caused by avoiding MM contents very few, and remanent magnetism and magnetic energy product performance caused by avoiding MM contents excessive
Be difficult to improve, and be more advantageous to and form a certain amount of richness MM phase structures in rare earth permanent magnet powder, to be more advantageous to entirety
The raising of magnetic property.
Meanwhile in rare earth permanent magnet powder provided by the invention, it is preferable that Ce contents are more than 48wt% in MM, and La contains in MM
Amount is more than 15wt%.Since each rare earth element is unevenly distributed (wherein, principal crystalline phase and richness MM phases in principal crystalline phase and richness MM phases
Middle Ce and Nd are evenly distributed, and La and Pr are more enriched in rich MM phases), to improve the magnetic property of the rare earth permanent magnet powder.
In rare earth permanent magnet powder provided by the invention, it is preferable that contain T in rare earth permanent magnet powder, wherein T be Co, Al, Zr and
Si any one or more ofs are calculated with the gross mass of rare earth permanent magnet powder key component, and the percentage composition of T is 0.32~
12.67wt%.Due to having a certain amount of T in rare earth permanent magnet powder, to promote being uniformly distributed for richness MM phases in crystal boundary, and
It can inhibit the microstructure segregation of each element in rich MM phases, and then not only miniaturization tissue but also improve the uniformity of structure.In order to
With former key component MMxFe1-x-yByEach ingredient preferably match, it is preferable that the mass ratio of T and Fe in rare earth permanent magnet powder is
0.5~10：100.In above-mentioned preferred range, it as can avoid the content of T very few as possible and lead to not uniform richness MM phases
Effect and content it is excessive and cause final magnetic property decline.It is further preferable that T and Fe in rare earth permanent magnet powder
Mass ratio is 0.5~5：100.The quality of above-mentioned preferred T and Fe can further increase the magnetism of rare earth permanent magnet powder than range
Energy.
In rare earth permanent magnet powder provided by the invention, it is preferable that the knee point coercivity and intrinsic coercivity of rare earth permanent magnet powder
Ratio >=70%.(i.e. rare earth permanent magnet powder is rectangular for the ratio of higher magnet knee point coercivity Hk and intrinsic coercivity Hcj
Degree) illustrate that the rare earth permanent magnet powder can overcome the more demagnetizing curve brought of each rare earth element in norium (MM) uneven
The problems such as sliding, so that the rare earth permanent magnet powder has higher whole magnetic property.
According to another aspect of the present invention, a kind of preparation method of rare earth permanent magnet powder is provided.The preparation method include with
Lower step：Master alloy is melted to form key component as MMxFe1-x-yByMolten alloy, wherein MM be mischmetal
Metal, x are 23~35wt.%, and y is 0.95~1.05wt.%；Rotation is carried out to molten alloy and quenches processing to form alloy powder；
And rotation cooling treatment is carried out to alloy powder to form rare earth permanent magnet powder, rare earth permanent magnet powder includes principal crystalline phase and is distributed in master
Rich MM phases around crystalline phase, principal crystalline phase MM2Fe14B phases, and the content of La is higher than the content of La in principal crystalline phase in richness MM phases, it is rich
The content of Pr is higher than the content of principal crystalline phase Pr in MM phases.
It is directly isolated from primary mineral products since the norium that is formed in above-mentioned rare earth permanent magnet powder has
The rare earth elements such as Nd, Ce and La, therefore the rare earth formed with the mixture by single rare earth metal and single rare earth metal is forever
Magnetic powder is compared, and rare earth permanent magnet powder provided by the invention drastically reduces the waste of rare earth resources, and norium has
The symbiotic characteristics of these rare earth elements make it have apparent synergistic effect, so as to make the rare earth permanent magnet powder to be formed show
Go out the magnetic property of single compound；Also, since the content of norium MM is 23%~35wt%, so as to
Make to form a certain amount of richness MM phase structures in the rare earth permanent magnet powder to be formed, richness MM phase structures can not only improve rare earth permanent magnet powder
Coercivity, and can become pinning sites of the rare earth permanent magnet powder in reverse magnetization process, to improve the rare earth permanent magnet
The magnetic property of powder, and then make the rare earth permanent magnet powder that there is higher cost performance.
The illustrative embodiments of the preparation method according to permanent-magnet material provided by the invention are described in more detail below.
However, these illustrative embodiments can be implemented by many different forms, and it should not be construed to be limited solely to this
In the embodiment that is illustrated.It should be understood that these embodiments are provided so that disclosure herein thoroughly and
Completely, and by the design of these illustrative embodiments those of ordinary skill in the art are fully conveyed to.
First, will carry out melting with the mixed metal of MM, Fe and the B mixed in proportion is to form key component
The master alloy of MMxFe1-x-yBy, wherein MM are norium, and x is 23~35wt.%, and y is 0.95~1.05wt%.Tool
Body, metal MM, Fe and B are mixed in proportion, wherein the ratio of MM, Fe and B are x：1-x-y：Y, and x be 23~
35wt.%, y are 0.95~1.05wt%；Then mixed metal is subjected to melting to form key component as MMxFe1-x-yBy
Master alloy.The technique of wherein melting may be used medium frequency induction melting furnace and carry out melting to be prepared into master alloy.
Preferably, Ce contents are more than 48wt% in MM, and La contents are more than 15wt% in MM.Since each rare earth element is in oikocryst
Uneven distribution in phase and richness MM phases, wherein Ce and Nd is evenly distributed in principal crystalline phase and richness MM phases, and La and Pr are more enriched with
In rich MM phases, so as to improve the magnetic property for the rare earth permanent magnet powder being subsequently formed.It is further preferable that x is 25~32wt%.When
When the content of MM is 25%~32wt%, coercitive decline caused by MM contents can be avoided very few, and MM is avoided to contain
Remanent magnetism and magnetic energy product performance are difficult to improve caused by amount is excessive, and are more advantageous in the rare earth permanent magnet powder for making to be subsequently formed
A certain amount of richness MM phase structures are formed, to be more advantageous to the raising of whole magnetic property, to improve the rare earth permanent magnet powder
Magnetic property.
It is preferred that containing T in above-mentioned rare earth permanent magnet powder, wherein T is any one of Co, Al, Zr and Si or more
Kind, it is calculated with the gross mass of rare earth permanent magnet powder key component, the percentage composition of T is 0.32~12.67wt%.Due to the master alloy
In there is a certain amount of T, to promote being uniformly distributed for richness MM phases in crystal boundary, and each element in rich MM phases can be inhibited
Microstructure segregation not only miniaturization tissue but also had improved the uniformity of structure.In order to former key component MMxFe100-x-yBy's
Each ingredient preferably matches, it is preferable that the mass ratio of T and Fe in the master alloy are 0.5~10：100.In above-mentioned preferred model
In enclosing, it as can avoid the content of T very few as possible and lead to not the effect of uniform richness MM phases and content excessively causes
The magnetic property of finally formed rare earth permanent magnet powder declines.
The mixed metal for having MM, Fe and B for mixing in proportion is being subjected to melting to form key component as MMxFe1-
After the step of master alloy of x-yBy, master alloy is melted to form molten alloy；Then, molten alloy is revolved
Processing quench to form alloy powder.Those skilled in the art can set the process conditions for revolving processing of quenching according to actual demand
It is fixed, in a preferred embodiment, molten alloy is sprayed onto on the roller of rotation and carries out revolving processing of quenching, the rotational line of roller
Speed is 20~35m/s.Above-mentioned preferred process conditions rotary speed can be avoided too low and caused by alloy powder crystal grain group
It knits coarse, to reduce the performance of final rare earth permanent magnet powder, while can also avoid speed excessively high and cause in alloy powder
A large amount of appearance of amorphous, and due to the step of not being heat-treated in subsequent technique, to which the rare earth of high magnetic characteristics can not be obtained
Permanent magnetism powder.
Meanwhile in above-mentioned preferred embodiment, the surfacing of roller can also be selected according to actual demand,
Preferably, roller surface is Mo or BeCu.Use above-mentioned material that can be more conducive in the processing step that processing is quenched in rotation
The stability for process of quenching is revolved, and then the rare earth permanent magnet powder of performance stabilization can be obtained in the subsequent process.
It completes after carrying out the step of rotation quenches processing to form alloy powder to molten alloy, alloy powder is rotated
Cooling treatment is to form rare earth permanent magnet powder, and rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, oikocryst
It is mutually MM2Fe14B phases, and in richness MM phases La content of the content higher than La in principal crystalline phase, the content of Pr is higher than oikocryst in rich MM phases
The content of phase Pr.Due to uneven distribution of each rare earth element in principal crystalline phase and richness MM phases, wherein in principal crystalline phase and richness MM phases
Ce and Nd are evenly distributed, and La and Pr are more enriched in rich MM phases, to improve the magnetic property of the rare earth permanent magnet powder.
The present invention directly obtains final rare earth permanent magnet powder by revolving to quench processing and rotate cooling treatment, does not include at heat
The processing step of reason, this is primarily due to contain a richness MM phases in rare earth permanent magnet powder provided by the invention, this is mutually in MM2Fe14B master
Be uniformly distributed outside crystalline phase, and in norium each element enrichment ratio it is different, after heat treatment step,
Even tissue makes the ingredient of principal crystalline phase and Grain-Boundary Phase be intended to balance, to obtain the rare earth permanent magnet powder of high magnetism.
Since the present invention is without being heat-treated, the stability between magnetic powder particle is particularly important to final magnetic property.
Rotation is quenched after the step of handling, and the alloy molten steel of melting is by being quickly cooled down and solidifying, but the flakelike powder obtained at this time still has
500 DEG C or so of temperature be easy to cause that local temperature is excessively high, and class occurs in part magnetic powder if directly allowing the powder accumulation to fly out
Like the process of heat treatment, it is unfavorable for the raising of entire magnetic property.And the step of rotating cooling treatment, can optimize entire flake powder
The cooling uniformity in end, to be conducive to the raising of the entire performance of rare earth permanent magnet powder, and then can ensure final magnetic powder tissue and
The uniformity of structure.Meanwhile those skilled in the art can carry out the process conditions for rotating cooling treatment according to actual demand
Setting, it is preferable that in carrying out the step of rotation cooling treatment is to form rare earth permanent magnet powder to alloy powder, the rotation of alloy powder
Rotary speed is less than 5m/s.The above-mentioned slower speed of rotation be conducive to entirely rotate cooling treatment during rare earth permanent magnet powder it is uniform
It is cooling.
Main phase provided by the present invention is MM2Fe14The rare earth permanent magnet powder of B structure, by the rare earth permanent-magnet powder and resin into
Row is mixed and made into isotropic bonded permanent magnet.Preparation method can be by prepared by the methods of molding, injection, calendering, extrusion
At.The bonded permanent magnet of preparation can be the other forms such as bulk, ring-type.
The bonded permanent magnet that the present invention obtains can be applied in the preparation of corresponding device.High property is prepared by the above method
The rare earth permanent magnet powder and magnet of energy, are conducive to miniaturising for device.
The rare earth permanent magnet powder of offer and the preparation side of rare earth permanent magnet powder are be provided below in conjunction with embodiment
Method.
Embodiment 1
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe and B are subjected to melting to form key component as MM30Fe69B
(MM30Fe69The concrete component of MM is as shown in table 1 in B) master alloy；Then master alloy is melted to form molten alloy；
Then rotation is carried out to molten alloy and quenches processing to form alloy powder, wherein the roller that institute's molten alloy is sprayed onto to rotation is enterprising
Row revolves processing of quenching, and the surface of roller is Mo layers, and the linear velocity of roller is 25m/s；Finally, alloy powder is revolved
Turn cooling treatment to form principal crystalline phase as MM2Fe14B phase rare earth permanent magnet powders, wherein rotation cooling treatment is carried out using chill roll,
The rotary speed of chill roll is 2m/s.Finally formed rare earth permanent magnet powder includes principal crystalline phase and the rich MM that is distributed in around principal crystalline phase
Phase, wherein principal crystalline phase are MM2Fe14B phases.Also, energy spectrum analysis is carried out using scanning electron microscope, as a result obtains containing for La in rich MM phases
Content of the amount higher than La in principal crystalline phase, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Embodiment 2
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe and B are subjected to melting to form key component as MM23Fe76.05B0.95
(MM23Fe76.05B0.95The concrete component of middle MM is as shown in table 1) master alloy；Then master alloy is melted to form melting
Alloy；Then rotation is carried out to molten alloy and quenches processing to form alloy powder, wherein institute's molten alloy is sprayed onto to the roller of rotation
On carry out rotation and quench processing, the surface of roller is Mo layers, and the linear velocity of roller is 20m/s；Finally, to alloy powder into
Row rotation cooling treatment is to form principal crystalline phase as MM2Fe14B phase rare earth permanent magnet powders, wherein carry out rotating cooling place using chill roll
The rotary speed of reason, chill roll is 1m/s.Finally formed rare earth permanent magnet powder includes principal crystalline phase and is distributed in around principal crystalline phase
Rich MM phases, wherein principal crystalline phase are MM2Fe14B phases.Also, energy spectrum analysis is carried out using scanning electron microscope, as a result obtains La in rich MM phases
Content of the content higher than La in principal crystalline phase, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Embodiment 3
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe, B and T are carried out melting is to form key component
MM25Fe73.63BT0.32(MM25Fe73.63BT0.37The concrete component of middle MM is as shown in table 1) master alloy, wherein T be Co, and T with
The mass ratio of Fe is 0.5：100；Then master alloy is melted to form molten alloy；Then rotation is carried out to molten alloy to quench
Processing is to form alloy powder, wherein institute's molten alloy is sprayed onto on the roller of rotation and carries out revolving processing of quenching, the surface of roller is
Mo layers, and the linear velocity of roller is 25m/s；Finally, rotation cooling treatment is carried out to form principal crystalline phase to alloy powder
For MM2Fe14B phase rare earth permanent magnet powders, wherein carry out rotation cooling treatment using chill roll, the rotary speed of chill roll is 2m/s.
Finally formed rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, and wherein principal crystalline phase is MM2Fe14B
Phase.Also, energy spectrum analysis is carried out using scanning electron microscope, as a result show that the content of La in rich MM phases contains higher than La in principal crystalline phase
It measures, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Embodiment 4
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe, B and T are carried out melting is to form key component
MM32Fe63.81BT3.19(MM32Fe63.81BT3.19The concrete component of middle MM is as shown in table 1) master alloy, wherein T be Co and Al, and
The mass ratio of T and Fe is 5：100；Then master alloy is melted to form molten alloy；Then molten alloy is revolved
Processing quench to form alloy powder, wherein institute's molten alloy is sprayed onto on the roller of rotation and carries out revolving processing of quenching, the surface of roller
It it is Mo layers, and the linear velocity of roller is 30m/s；Finally, rotation cooling treatment is carried out to form oikocryst to alloy powder
It is mutually MM2Fe14B phase rare earth permanent magnet powders, wherein carry out rotation cooling treatment using chill roll, the rotary speed of chill roll is 3m/
s.Finally formed rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, and wherein principal crystalline phase is
MM2Fe14B phases.Also, energy spectrum analysis is carried out using scanning electron microscope, as a result obtains the content of La in rich MM phases higher than in principal crystalline phase
The content of La, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Embodiment 5
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe, B and T are carried out melting is to form key component
MM35Fe58.14B1.05T5.81(MM35Fe58.14B1.05T5.81The concrete component of middle MM is as shown in table 1) master alloy, wherein T be Co,
Al and Si, and the mass ratio of T and Fe is 10：100；Then master alloy is melted to form molten alloy；Then to melting
Alloy carries out rotation and quenches processing to form alloy powder, wherein and institute's molten alloy is sprayed onto on the roller of rotation and carries out revolving processing of quenching,
The surface of roller is BeCu layers, and the linear velocity of roller is 35m/s；Finally, alloy powder is carried out rotating cooling place
Reason is to form principal crystalline phase as MM2Fe14B phase rare earth permanent magnet powders, wherein rotation cooling treatment is carried out using chill roll, chill roll
Rotary speed is 4m/s.Finally formed rare earth permanent magnet powder includes principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, wherein
Principal crystalline phase is MM2Fe14B phases.Also, energy spectrum analysis is carried out using scanning electron microscope, as a result show that the content of La in rich MM phases is higher than
The content of La in principal crystalline phase, the content of Pr is higher than the content of principal crystalline phase Pr in rich MM phases.
Embodiment 6
The preparation process of rare earth permanent magnet powder provided in this embodiment includes：
First, the mixed metal of mixed MM, Fe, B and T are carried out melting is to form key component
MM35Fe51.28B1.05T12.67(MM35Fe51.28B1.05T12.67The concrete component of middle MM is as shown in table 1) master alloy, wherein T be Co,
Al, Zr and Si；Then master alloy is melted to form molten alloy；Then rotation is carried out to molten alloy and quenches processing to be formed
Alloy powder, wherein institute's molten alloy is sprayed onto on the roller of rotation and revolve processing of quenching, the surface of roller is BeCu layers, and
And the linear velocity of roller is 35m/s；Finally, carry out rotation cooling treatment to alloy powder is to form principal crystalline phase
MM2Fe14B phase rare earth permanent magnet powders, wherein carry out rotation cooling treatment using chill roll, the rotary speed of chill roll is 4m/s.Most
End form at rare earth permanent magnet powder include principal crystalline phase and the rich MM phases that are distributed in around principal crystalline phase, wherein principal crystalline phase is MM2Fe14B phases.
Also, energy spectrum analysis is carried out using scanning electron microscope, as a result obtains content of the content higher than La in principal crystalline phase of La in rich MM phases, it is rich
The content of Pr is higher than the content of principal crystalline phase Pr in MM phases.
Comparative example 1
The preparation process of permanent-magnet material that this comparative example provides includes：
First, the master alloy being made of elemental cerium, iron and boron is prepared；Then master alloy is melted and is with forming component
Ce15.4Fe76.9B7.7Molten alloy；Then added by the way that the stream of molten alloy to be directed on the surface of rotating metallic wheel
Work, by molten alloy flow quenching at graininess alloy composite；Alloy composite is subjected to high annealing with shape at 500 DEG C
It is Ce at principal crystalline phase2Fe14The permanent-magnet material of B.
MM in the rare earth permanent magnet powder that embodiment 1 to 6 is providedxFe1-x-yBy(or MMaFe1-a-b-cBbTc) in specific group of MM
Divide (i.e. the weight percent that each metallic element accounts for MM in MM) as shown in table 1；In the rare earth permanent magnet powder that embodiment 3 to 6 is provided
MMaFe1-a-b-cBbTcThe concrete component (i.e. each metallic element accounts for the weight percent of T in T) of middle T is as shown in table 2.
Table 1
Table 2
| No. | Co wt% | Al wt% | Si wt% | Zr wt% |
| Embodiment 3 | 0.37 | 0 | 0 | 0 |
| Embodiment 4 | 2.13 | 1.06 | 0 | 0 |
| Embodiment 5 | 1.6 | 2.14 | 2.07 | 0 |
| Embodiment 6 | 2.56 | 3.43 | 3.27 | 3.41 |
The present invention is also tested for the squareness for the rare earth permanent magnet powder that embodiment 1 to embodiment 6 and comparative example 1 is provided (i.e.
The ratio of knee point coercivity and intrinsic coercivity) and maximum magnetic energy product, the results are shown in Table 3.
Table 3
From table 1, table 2 and table 3 as can be seen that the squareness and maximum of the rare earth permanent magnet powder that 1~embodiment of embodiment 6 provides
Magnetic energy product is significantly greater than the rare earth permanent magnet powder that comparative example 1 provides, therefore the sample of 1~embodiment of embodiment 6 achieves preferably
Magnetic property.
In addition, according to the present invention, the rare earth permanent magnet powder that can be used to is mixed with binder to carry out bonding and prepares bonded permanent magnet,
It is applied in occasions such as motor, sound equipment, measuring instruments.
It can be seen from the above description that the above embodiments of the present invention realize following technique effect：The present invention carries
It is MM to have supplied a kind of key componentxFe1-x-yByRare earth permanent magnet powder, since the norium in the rare earth permanent magnet powder has
The rare earth elements such as Nd, Ce and the La directly isolated from primary mineral products, thus with by single rare earth metal and single dilute
The rare earth permanent magnet powder of the mixture composition of earth metal is compared, and rare earth permanent magnet powder provided by the invention drastically reduces rare earth resources
Waste, and the symbiotic characteristic of these rare earth elements that norium has makes it have apparent synergistic effect, to
Rare earth permanent magnet powder can be made to show the magnetic property of single compound；Also, since the MM contents in the rare earth permanent magnet powder are
23%~35wt%, to make to form a certain amount of richness MM phase structures in rare earth permanent magnet powder, richness MM phase structures can not only
The coercivity of rare earth permanent magnet powder is improved, and pinning sites of the rare earth permanent magnet powder in reverse magnetization process can be become, to carry
The high magnetic property of the rare earth permanent magnet powder, and then make the rare earth permanent magnet powder that there is higher cost performance.
It these are only the preferred embodiment of the present invention, be not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification made by all within the spirits and principles of the present invention,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (13)
1. a kind of rare earth permanent magnet powder, which is characterized in that the key component of the rare earth permanent magnet powder is MMxFe1-x-yBy, wherein MM is
Norium, x are 23~35wt%, and y is 0.95~1.05wt%；The rare earth permanent magnet powder includes principal crystalline phase and is distributed in
Rich MM phases around the principal crystalline phase, the principal crystalline phase are MM2Fe14B phases, and the content of La is higher than the master in the richness MM phases
The content of La in crystalline phase, the content of Pr is higher than the content of the principal crystalline phase Pr in the richness MM phases, Ce in principal crystalline phase and richness MM phases
It is evenly distributed with Nd.
2. rare earth permanent magnet powder according to claim 1, which is characterized in that Ce contents are more than 48wt% in MM, and La contains in MM
Amount is more than 15wt%.
3. rare earth permanent magnet powder according to claim 1, which is characterized in that contain T in the rare earth permanent magnet powder, wherein T is
Co, Al, Zr and Si any one or more of are calculated, the percentage composition of T with the gross mass of the rare earth permanent magnet powder key component
For 0.32~12.67wt%.
4. rare earth permanent magnet powder according to claim 3, which is characterized in that the quality of T and Fe in the rare earth permanent magnet powder
Than being 0.5~10：100.
5. rare earth permanent magnet powder according to claim 4, which is characterized in that the quality of T and Fe in the rare earth permanent magnet powder
Than being 0.5~5：100.
6. a kind of preparation method of rare earth permanent magnet powder, which is characterized in that the preparation method comprises the following steps：
Melting will be carried out to form key component as MM with the mixed metal of MM, Fe and the B mixed in proportionxFe1-x-yByMother
Alloy, wherein MM are norium, and x is 23~35wt.%, and y is 0.95~1.05wt%；
The master alloy is melted to form molten alloy；
Rotation is carried out to the molten alloy and quenches processing to form alloy powder；And
Rotation cooling treatment is carried out to form the rare earth permanent magnet powder to the alloy powder, the rare earth permanent magnet powder includes oikocryst
Phase and the rich MM phases being distributed in around the principal crystalline phase, the principal crystalline phase are MM2Fe14B phases, and in the richness MM phases La content
Higher than the content of La in the principal crystalline phase, in the richness MM phases content of Pr be higher than the principal crystalline phase Pr content, principal crystalline phase and
Ce and Nd is evenly distributed in rich MM phases.
7. preparation method according to claim 6, which is characterized in that the roller that the molten alloy is sprayed onto to rotation is enterprising
Row is described to revolve processing of quenching, and the linear velocity of the roller is 20~35m/s.
8. preparation method according to claim 7, which is characterized in that the surface of the roller is Mo layers or BeCu layers.
9. preparation method according to claim 6, which is characterized in that carrying out rotation cooling treatment to the alloy powder
With in the step of forming the rare earth permanent magnet powder, the rotary speed of the alloy powder is less than 5m/s.
10. preparation method according to claim 6, which is characterized in that in the step of being melted the master alloy,
The master alloy further includes T, and wherein T is Co, Al, Zr and Si any one or more of, with the main group of the rare earth permanent magnet powder
The gross mass divided calculates, and the percentage composition of T is 0.32~12.67wt%.
11. preparation method according to claim 10, which is characterized in that the mass ratio of T and Fe is 0.5 in the master alloy
~10：100.
12. a kind of bonded permanent magnet, which is characterized in that the bonded permanent magnet be rare earth described in any one of claim 1 to 5 forever
Magnetic powder is bonded with binder.
13. a kind of device, which is characterized in that the device applies the bonded permanent magnet described in claim 12.
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|---|---|---|---|---|
| CN1234589A (en) * | 1998-03-23 | 1999-11-10 | 住友特殊金属株式会社 | Permanent magnet and R-TM-B series permanent magnet |
| CN102376407A (en) * | 2010-07-27 | 2012-03-14 | Tdk株式会社 | Rare earth sintered magnet |
| CN103035350A (en) * | 2013-01-10 | 2013-04-10 | 浙江大学 | Low-cost permanent magnet prepared from misch metal (MM) and preparation method thereof |
| CN104078176A (en) * | 2013-03-28 | 2014-10-01 | Tdk株式会社 | Rare earth based magnet |
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| JP3642781B2 (en) * | 2003-09-25 | 2005-04-27 | Ｔｄｋ株式会社 | R-T-B permanent magnet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234589A (en) * | 1998-03-23 | 1999-11-10 | 住友特殊金属株式会社 | Permanent magnet and R-TM-B series permanent magnet |
| CN102376407A (en) * | 2010-07-27 | 2012-03-14 | Tdk株式会社 | Rare earth sintered magnet |
| CN103035350A (en) * | 2013-01-10 | 2013-04-10 | 浙江大学 | Low-cost permanent magnet prepared from misch metal (MM) and preparation method thereof |
| CN104078176A (en) * | 2013-03-28 | 2014-10-01 | Tdk株式会社 | Rare earth based magnet |
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